scholarly journals Development and validation of a simple bio-analytical HPLC-UV method for estimation of irbesartan in human plasma

2020 ◽  
Vol 11 (3) ◽  
pp. 3846-3849
Author(s):  
Ashok P ◽  
Narenderan S T ◽  
Meyyanathan S N ◽  
Babu B ◽  
Jawahar N
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
High Performance ◽  
Internal Standard ◽  
Precipitation Method ◽  
Quantification Limit ◽  
Us Fda ◽  
Development And Validation ◽  
Analytical Hplc

The present study was aimed to develop and validate a simple, sensitive and economical bio-analytical high-performance liquid chromatographicultraviolet method for the determination of irbesartan in human plasma. The method involves the use of simple precipitation method for the determination of irbesartan, using methanol as precipitating agent and losartan as internal standard. The separation was achieved using Zorbax C18 column (150 x 4.6 mm, 5µm), mobile phase consists of methanol and 0.2% formic acid in water at the ratio 85:15, v/v using detection wavelength of 237 nm. Further, the developed method was validated as per US-FDA guidelines for accuracy, precision, linearity, stability, detection and quantification limit. The method developed was found to be linear over the concentration ranging from 5 to 500 ng/ml with a correlation coefficient of 0.9987. The LOD and LLOQ of the method were found to be 1 ng/ml and 5 ng/ml, respectively.

scholarly journals Development and validation of a SPE-UHPLC-fluorescence method for the analysis of ochratoxin-a in certain Turkish wines

2019 ◽  
Vol 38 (2) ◽  
pp. 161
Author(s):  
Elif Mine Oncu Kaya
Keyword(s):  
Ochratoxin A ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Internal Standard ◽  
Fluorescence Method ◽  
Limit Of Quantitation ◽  
Development And Validation

A sensitive Ultra-High Performance Liquid Chromatography (UHPLC)-fluorescence method was developed and validated for the determination of ochratoxin-A (OTA) in Turkish wine samples. Naphthalene was used as an internal standard in this study. OTA was separated on a C18 (3.0 mm × 100 mm × 1.8 µm) column and analyses were run under isocratic conditions, with a mobile phase consisting of water/acetonitrile/acetic acid (50:50:1, v/v/v). The flow rate and injection volume were 0.5 ml min−1 and 10 μl, respectively. The excitation and emission wavelengths were 330 nm and 460 nm for OTA, respectively, and 220 nm and 325 nm for internal standard, respectively. A solid-phase extraction (SPE) clean-up procedure on a C18 cartridge was used prior to the analysis of the wine samples by UHPLC. The developed method was validated with respect to linearity, precision, accuracy, limit of detection (LOD), limit of quantitation (LOQ), stability and robustness. The method presented good RSD (< 4 %) and recovery (102.6–105.2 %) values. The LOD and LOQ values were 0.01 ng ml–1 and 0.05 ng ml–1, respectively. All other parameters were acceptable. OTA amounts were found in the range of 2.72‒7.40 µg kg‒1 in the Turkish wine samples.

scholarly journals High-Performance Liquid Chromatographic Determination of Proquazone and Its m-Hydroxy Metabolite in Spiked Human Plasma and Urine

2007 ◽  
Vol 90 (4) ◽  
pp. 971-976
Author(s):  
Ekram M Hassan ◽  
Azza A Gazy ◽  
Mohamed H Abdel-Hay ◽  
Tarek S Belal
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
High Performance ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Urine Samples ◽  
Spiked Human Plasma ◽  
Liquid Chromatographic ◽  
Hydroxy Metabolite

Abstract A simple and rapid high-performance liquid chromatographic method for the determination of proquazone (PQZ) and its major metabolite, m-hydroxyproquazone, in spiked human plasma and urine was developed. Plasma samples were purified using acetonitrile as a protein precipitant, while urine samples were diluted only with the mobile phase and filtered prior to injection. Samples containing the parent compounds and glafenine (internal standard) were eluted from a reversed-phase C8 column using acetonitrile-0.025 M sodium acetate (60 + 40) adjusted to pH 5 as the mobile phase and detected at 234 nm. Peak area ratios of the analytes versus internal standard were used for calibration. The mean recoveries from plasma and urine samples spiked with PQZ and its m-hydroxy metabolite ranged from 97.87 to 103.88%. The relative standard deviation for the within- and between-day analyses were &lt;4%. The proposed method was applied for the assay of PQZ in laboratory-made tablets.

scholarly journals Development and Validation of a High-Performance Liquid Chromatographic Method for the Determination of Cinitapride in Human Plasma

2018 ◽  
Vol 2018 ◽  
pp. 1-5
Author(s):  
Boovizhikannan Thangabalan ◽  
Getu Kahsay ◽  
Tadele Eticha
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Chromatographic Method ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Us Fda ◽  
Development And Validation ◽  
Liquid Chromatographic

A precise and reliable reversed-phase high-performance liquid chromatographic method with ultraviolet detection was developed and validated to determine cinitapride in human plasma. After liquid-liquid extraction, chromatographic separation was achieved on a Nucleosil C18 (25 cm × 4.6 mm, 5 µm) column with an isocratic elution consisting of 10 mM ammonium acetate (pH 5.2), methanol, and acetonitrile, 40 : 50 : 10, v/v/v. The developed method was validated as per US FDA guidelines for its linearity, selectivity, sensitivity, precision, accuracy, and stability. Satisfactory findings were obtained from the validation studies. The linearity range of the method was 1 to 35 ng/mL while the extraction recovery of cinitapride in human plasma was more than 86%. The percent coefficient of variation of both intraday and interday precision was ≤7.1%.

A Sensitive LC–MS/MS Method for the Determination of Afatinib in Human Plasma and Its Application to a Bioequivalence Study

2021 ◽  
Author(s):  
Xi Luo ◽  
Xiu Jin Zhang ◽  
Wen Ling Zhu ◽  
Jin Ling Yi ◽  
Wen Gang Xiong ◽  
...  
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Bioequivalence Study ◽  
Liquid Chromatography Tandem Mass ◽  
Multiple Reaction Monitoring Mode ◽  
Ionization Mode

Abstract A high performance liquid chromatography–tandem mass spectrometry assay for the determination of afatinib (AFT) in human plasma was established. A simple sample preparation of protein precipitation was used and separation was achieved on a C18 column by the gradient mixture of mobile Phase A of water (containing 0.1% ammonia) and the mobile Phase B of acetonitrile and water (V:V = 95:5, containing 0.2% ammonia). The multiple reaction monitoring mode was used to monitor the precursor-to-production transitions of m/z 486.2 → m/z 371.4 for AFT and m/z 492.2 → m/z 371.3 for AFT-d6 (internal standard) at positive ionization mode. The calibration curve ranged from 0.100 to 25.0 ng·mL−1 and the correlation coefficient was greater than 0.99. The intra- and inter-batch precision was less than or equal to 10.0%. Accuracy determined at four concentrations was in the range of 92.3–103.3%. In summary, our method was sensitive, simple and reliable for the quantification of AFT and was successfully applied to a bioequivalence study.

scholarly journals Development and validation of high-performance liquid chromatographic method for determination of ofloxacin and lomefloxacin in human plasma

2005 ◽  
Vol 70 (12) ◽  
pp. 1451-1460 ◽  
Author(s):  
Dragica Zendelovska ◽  
Trajce Stafilov
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Organic Modifiers ◽  
Liquid Chromatographic Method ◽  
Water Ph ◽  
Development And Validation ◽  
Liquid Chromatographic

Ahigh-performance liquid chromatographicmethod for the determination of ofloxacin and lomefloxacin in human plasma has been developed and validated. The effect of organic modifiers on the retention of the investigated drugs was investigated. A simple isocratic chromatographic assay with UV-detection at 280nm was performed on a Hibar Lichrospher 100 RP 8 column (250x4.6mm 5?m. Merck, Germany) using a mixture of acetonitrile and 0.5 % triethylamine in water (pH adjusted to 2.5 with H3PO4) (15:85, V/V) as the mobile phase at flow rate of 1.2 mL min-1. The calibration curves were linear in the concentration ragne of 0.5-6.0?g mL-1 for ofloxacin and 0.2-4.5 ?g mL-1 for lomefloxacin.

scholarly journals Bioanalytical method development and validation for determination of metoprolol tartarate and hydrochlorothiazide using HPTLC in human plasma

2013 ◽  
Vol 49 (4) ◽  
pp. 845-851 ◽  
Author(s):  
Ambadas Ranganath Rote ◽  
Poonam Ramdas Sonavane
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Method Development ◽  
Internal Standard ◽  
Analytical Technique ◽  
Method Development And Validation ◽  
Rf Values ◽  
The Stability ◽  
Development And Validation

A simple, sensitive, rapid and economic chromatographic method has been developed for determination of metoprolol tartarate and hydrochlorothiazide in human plasma using paracetamol as an internal standard. The analytical technique used for method development was high-performance thin-layer chromatography. HPTLC Camag with precoated silica gel Plate 60F254 (20 cm×10 cm) at 250 µm thicknesses (E. Merck, Darmstadt, Germany) was used as the stationary phase. The mobile phase used consisted of chloroform: methanol: ammonia (9:1:0.5v/v/v). Densitometric analysis was carried out at a wavelength of 239 nm. The rf values for hydrochlorothiazide, paracetamol and metoprolol tartarate were 0.13±0.04, 0.28±0.05, 0.48±0.04, respectively. Plasma samples were extracted by protein precipitation with methanol. Concentration ranges of 200, 400, 600, 800, 1000, 1200 ng/mL and 2000, 4000, 6000, 8000, 10000, 12000 ng/mL of hydrochlorothiazide and metoprolol tartarate, respectively, were used with plasma for the calibration curves. The percent recovery of metoprolol tartarate and hydrochlorothiazide was found to be 77.30 and 77.02 %, respectively. The stability of metoprolol tartarate and hydrochlorothiazide in plasma were confirmed during three freeze-thaw cycles (-20 ºC) on a bench for 24 hours and post-preparatively for 48 hours. The proposed method was validated statistically and proved suitable for determination of metoprolol tartarate and hydrochlorothiazide in human plasma.

The Dtermination of Paracetamol by HPLC Validation of the Method and Application on Serum Samples

2018 ◽  
Vol 69 (3) ◽  
pp. 627-631 ◽  
Author(s):  
Viorica Ohriac (Popa) ◽  
Diana Cimpoesu ◽  
Adrian Florin Spac ◽  
Paul Nedelea ◽  
Voichita Lazureanu ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Hplc Analysis ◽  
Emotional Experience ◽  
Optimum Conditions ◽  
Serum Samples ◽  
Liquid Chromatograph ◽  
Mobile Phase Flow Rate ◽  
Quantification Limit

Pain is defined as a disagreeable sensory and emotional experience related to a tissue or potential lesion. Paracetamol (Acetaminophen) is the most used non-morphine analgesic. For the determination of paracetamol we developed and validated the high performance liquid chromatography (HPLC) analysis using a Dionex Ultimate 3000 liquid chromatograph equipped with a multidimensional detector. After determining the optimum conditions of analysis (80/20 water / acetonitrile mobile phase, flow rate 1.0 mL / min, detection wavelength 245 nm) we validated the method following the following parameters: linearity of response function, linearity of results, limit (LD = 0.66 mg / mL) and quantification limit (LQ = 2.00 mg / mL), and precision. The method of determining paracetamol by HPLC was applied to 30 samples of serum collected from patients who had pain and were treated with paracetamol.

Development and Validation of an LC-MS/MS Method for Simultaneous Determination of Canagliflozin and Metformin HCl in Rat Plasma and its Application

2020 ◽  
Vol 16 (6) ◽  
pp. 752-762
Author(s):  
Vivek Nalawade ◽  
Vaibhav A. Dixit ◽  
Amisha Vora ◽  
Himashu Zade
Keyword(s):  
Internal Standard ◽  
Rat Plasma ◽  
Precipitation Method ◽  
Herbal Extracts ◽  
One Step ◽  
Precision And Accuracy ◽  
Development And Validation ◽  
The Impact ◽  
Metformin Hcl

Background: Food and herbal extracts rich in Quercetin (QRT) are often self-medicated by diabetics and can potentially alter the pharmacokinetics (PK) of Metformin HCl (MET) and Canagliflozin (CNG) leading to food or herb-drug interactions and reduced therapeutic efficacy. However, the impact of these flavonoids on the pharmacokinetic behaviour of MET and CNG is mostly unknown. Methods: A simple one-step protein precipitation method was developed for the determination of MET and CNG from rat plasma. The mobile phase chosen was MeOH 65% and 35% water containing 0.1% formic acid at a flow rate of 1mL/min. Results: The retention time of MET, internal standard (Valsartan) and CNG was 1.83, 6.2 and 8.2 min, respectively. The method was found to be linear in the range of 200 - 8000 ng/mL for CNG and 100 = 4000 ng/ml for MET. Precision and accuracy of the method were below 20% at LLOQ and below 15% for LQC, MQC, and HQC. Conclusion: The method was successfully applied for the determination of PK of MET and CNG by using 100 μL of rat plasma. QRT co-administration affects the PK parameters of MET and CNG. This alteration in PK parameters might be of significant use for clinicians and patients.

scholarly journals High-performance liquid chromatographic determination of famotidine in human plasma using solid-phase column extraction

2003 ◽  
Vol 68 (11) ◽  
pp. 883-892 ◽  
Author(s):  
Dragica Zendelovska ◽  
Trajce Stafilov
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Solid Phase ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Water Ph ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

A rapid, specific and sensitive high-performance liquid chromatographic method for the determination of famotidine in human plasma has been developed. Famotidine and the internal standard were chromatographically separated from plasma components using a Lichrocart Lichrospher 60 RP select B cartridge for solid-phase separation with a mobile phase composed of 0.1 % (v/v) triethylamine in water (pH 3) and acetonitrile (92:8, v/v). UV detection was set at 270 nm. The calibration curve was linear in the concentration range of 10.0 ? 350.0 ng mL-1. The method was implemented to monitor the famotidine levels in patient samples.

scholarly journals Bioanalytical Method Development and Validation for Determination of Sulfasalazine in Rabbit Plasma by HPLC-UV

2021 ◽  
Vol 33 (7) ◽  
pp. 1692-1698
Author(s):  
S.S. Jadiya ◽  
N. Upmanyu ◽  
S. Arulmozhi ◽  
V. Jain ◽  
S. Sankaran ◽  
...  
Keyword(s):  
High Performance ◽  
Method Development ◽  
High Efficiency ◽  
Internal Standard ◽  
Ultra Violet ◽  
Precipitation Method ◽  
Pharmacokinetic Studies ◽  
Rabbit Plasma ◽  
Bioanalytical Method

In present study, an advanced, simple and a rapid reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the quantitative determination of sulfasalazine in rabbit plasma. Sulfasalazine was separated using Chromatopak C-18 basic peerless (250 mm × 4.6 mm, 5μ) column in an isocratic mode using mobile phase consisting of the mixture of 10mM Ammonium acetate pH adjusted to 4.5 and acetonitrile (70:30 v/v) with a flow rate of about 1.0 mL/min at ambient temperature. An ultra-violet detection of sulfasalazine and the internal standard was carried out at 362 nm. Both sulfasalazine and internal standard (IS, 4-hydroxy benzoate) were extracted from plasma matrices with high efficiency using a simple protein precipitation method. The method was found to be highly selective with no carryover effects. Linearity of sulfasalazine was found with the range of 2.5-100 μg/mL with the value of r2 > 0.995 a correlation coefficient. At all three quality control levels, developed bioanalytical method was found as repeatable and reproducible as well. The average recoveries of sulfasalazine from plasma were in the range of 95.59-97.16%. The bioanalytical samples showed good and acceptable stability of sulfasalazine solution at different storage, packaging and handling conditions. Hence, in conclusion, the validated and developed HPLC-UV method could be effectively utilized for determination of sulfasalazine in pharmacokinetic studies involving novel formulations.

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